Method of using dilatable sealing elements



Aug. 21, 1 G. R. LUCAS ET AL 5 3 METHOD OF USING DILATABLE SEALING ELEMENTS Filed Aug. 17, 1946 Fig.1. Fig. 2.

TUBULHR Mf/YBER Fig.3.

705ml? MEMBER sEnu lva ELEMENT Inventors: Glennard R. Lucas, Richard QB gan.

Their Attorney.

i atented Aug. 21, 19 51 "UNITED STATES PATENT OFFICE METHOD OF USING DILATABLE SEALING ELEMENTS Glennard R. Lucas and Richard C. Bryan, Pittsfield, Mass, assignors to General Electric Company, a corporation of New York Application August 17, 1946, Serial No. 691,403

1 Claim.

. ,7 1 This invention relates to dilatablesealing elements and their manufacture by extrusion of polyvinyl chloride plastic compositions which are readilyextruded and yet capable of affording rigid, tightly-gripping sealing elements; and to a method of sealing openings with such elements.

The claims of the present application are directed particularly to the method of sealing openings with such elements while claims to the seals and their preparation are presented in our divisional application Serial No. 108,422, filed August 3, 1949, and assigned to the same assignee as" the present invention.

The sealing elements may be in the form of tubes for" connecting lengths of, for example,

tubin formed of other plastic material, or of glass, metal, etc. lengths of tubes sealed at one end for securely closing the ends of tubing or pipe; closures for bottles, etc.; or any other configuration which might be employed as a dilatable sealing element.

After extrusion to the desired shape, the elements. are expanded by immersion in a dilater liquid which penetrates the polyvinyl chloride plastic, causing the elements to soften slightly and expand, thus facilitating placing the elements on the tubes, bottles, etc., which it is desired to seal.f The composition of the dilater liquid will hereinafter be described in more detail. After the sealin elements are in place, the dilater is allowed to escape either slowly at room temperature and prevailing atmospheric pressure; or more rapidly at elevated temperatures Or reduced pressure or a combination of both conditions. the sealing elements to shrink to the final desired dimensions and grip tightly the openings of the tubes or other shapes to which they have been applied.

The general process is illustrated in the accompanying drawing in which Fig. 1 shows a plastic sealing element which may be used in the practice of the invention with reference to the closing of an end of a tube; Fig. 2 shows a tubular member the end of which is to be sealed by the sealing element; Fig. 3 shows the sealing element in the expanded form ready to be placed upon the end of the tubular member; and Fig. 4 illustrates the sealing element shrunk into sealing relationship with the end of the tubular member after placing the element on the end of the tubular member.

Heretofore it has been well known to extrude polyvinyl chloride compositions containin appreciable quantities of plasticizers such as tricresyl' phosphate, dioctyl phthalate, and other high boiling compounds. compatible with and. capable of .plasticiz'in polyvinyl chloride resins. The. addition of these plasticizers :to polyvinyl Escape of the dilater causeschloride has been necessary to produce compositions which are extrudable at temperatures below the decomposition temperature of the polyvinyl chloride and which are capable of affording tough, well-knit, extruded shapes. Because of the relativelyhigh softening points of polyvinyl chloride, it has been necessary in the past to work the plasticizer and resin into an extrudable material by means of masticating rolls, and to sheet the resulting rubbery plastic mass. The plastic sheet must then be shredded in order to be handled in subsequent extrusion operations.

In many applications, the presence of the normally appreciable quantities of plasticizer in the final extruded polyvinyl chloride shapes is very undesirable. Thus, when conventional, highly plasticized polyvinyl chloride compositions are employed in the manufacture of extruded sealing elements, the rigidity of the final sealing element may not be sufficient to afford the desired security in the seal. Furthermore, because of the nature of the dispersion of ordinary plasticizers in the polyvinyl chloride resin, there is a tendency for sealng elements to become more pervious as plasticizer is leached out by the dilater liquid.

It is, therefore, one of the objects of this invention to provide a method for the manufacture of dilatable polyvinyl chloride plastic sealil'lg elements of sufficient rigidity to insure dimensionally stable and secure seals.

Another object of the invention is to provide a simplified method of preparing an extrudable polyvinyl chloride plastic composition in which the steps of masticating on rolls and shredding preparatory to extrusion are unnecessary. Other objects of the invention will be apparent to those skilled in the art as a reading of this specification proceeds.

In preparing the extrudable polyvinyl chloride plastic composition, the dry ingredients comprising a polyvinyl chloride composition Such as, for example, polymers commercially available as Geon RF-IOO or Geon 102 are first mixed thoroughly in a suitable mixer such as a Baker- Perkins type mixer. If it is desired to obtain transparent sealing elements, no pigments or fillers are added. However, for opaque or colored elements, fillers and pigments such as, for example, zinc oxide and reen chrome oxide are mixed with the polyvinyl chloride composition. If transparent, colored sealing elements are desired, as where a problem of identification is involved, an organic dye may be added instead of the fillers or colored pigments. A-stabilizer for the polyvinyl chloride resin may also be mixed With the other dry ingredients. The addition of a suitable stabilizer such as, for example, litharge or lead silicate in amounts of from about two to five percent by weight of the polyvinyl chloride resin has been found to be desirable for stabilizing the polyvinyl chloride during the extrusion of the plastic composition. Various ratios of fillers and colored pigments to polyvinyl chloride may be employed. However, particularly satisfactory results have been obtained when the ratio by weight of the filler and colored pigment to the resin is about one to one.

After the dry ingredients (ingredients not liquid at ordinary conditions of temperature and pressure) have been thoroughly mixed, a temporary plasticizer is added with continued mixing. The term temporary plasticizer as used herein refers to compounds or mixtures of compounds which are compatible with polyvinyl chloride resin and which may be removed in part or entirely, either during immersion in the dilater, or during operations after extrusion or application to the object to be sealed, without aiiecting the impervious nature of the sealing element. Such temporary plasticizers are to be distinguished from the ordinary type of high-boiling plasticizers which it is necessary to retain almost entirely in the plastic even after it has been molded into its final form.

In general, the plasticizers employed in the method ofthis invention comprise mixtures of a solvent for polyvinyl chloride resin and a nonsolvent for the resin. Suitable solvents are ketones, for example, isophorone, mesityl oxide, ienchone, cyclohexanone, methyl butyl ketone, methyl isobutyl ketone, methyl amyl ketone, methyl isoamyllretone, ethyl amyl ketone, etc. Suitable non-solvents are materials in which polyvinyl chloride is insoluble and, in addition, certain materials in which polyvinyl chloride is slightly soluble only at elevated temperatures. Examples of suitable non-solvents are aromatic hydrocarbons andhalogenated aromatic hydrocarbons, for example, xylene, dichlorobenzene, monochlorotoluene, diethylbenzene, chlorinated xylenes, etc.

Various ratios of solvents to non-solvents may be employed in the temporary plasticizer. It has been found that when a solvent alone is addedto the mixture of resin and-filler as a plasticizer, a rubbery mass results which is diiiicult to work in the mixer and which cannot readily be handled in an extruder. non-solvent to the mixture, the mass tends to form a gel-like product which is readily mixed and broken up into small particles that are easily handled in an extrusion machine or other forming device.

Various combinations ofsolvents and nonsolvents may be employed. However, we have found that mixtures ,of isophorone and monochlorotoluene afford particularly good results when employed in accordance with the method of our invention. The ratio by weight of isophorone to monochlorotoluene should preferably be one part of isophorone to from approximately two to three parts of monochlorotoluene. The amount of temporary plasticizer added to the dry ingredients may be varieddepending, for example, on the shape of the sealing elements to be extruded. However, the addition of temporary plasticizer in amounts approximately equal by weight to the weight of polyvinyl chloride resin has been found to be suitable for most applications.

For certain applications it may be desirable to obtain sealing elements having less rigidity than that ultimatelyobtainable by employing compositions prepared in accordance with the However, by adding suiiicient method set forth above. More flexible sealing elements may be obtained by the addition of small quantities of high boiling plasticizers, e. g., tricresyl phosphate, dioctyl phthalate, etc., to the mass during the mixing operation.

After the dry ingredients and the plasticizer have been thoroughly mixed, and while continuing mixing, su'fficient' heat is applied to the mixer to raise the temperature of the mass to from about 40 to C. When the mass begins to stiffen up, it is cooled rapidly and mixing is continued until the mass is broken up into small rubbery curds. These curds can be stored for long periods of time without agglomerating into larger lumps. This is an advantage which cannot be obtained if the temporary plasticizer contains only compounds which are solvents for the polyvinyl chloride. resin.

The plastic composition in the form of rubbery curds may be stored in drums for subsequent use, or it may be transferred directly to a forming device such as for instance, an extruder, for forming into the desired shapes for sealing elements.

By employin temporary plasticizers such as, for example, an isophorone-monochlorotoluene mixture, it is possible to prepare an extruda-ble composition by ordinary mixing methods, thus eliminating the necessity vfor mixing on. rolls which is normally incident to the preparation of compositions. containing the usual high boiling plasticizers. In addition, the product is in the. form of rubberycurds which are readily handled in the extruder without intermediate processing. In the method heretofore employed it has been necessary to put the sheet. plastic from the masticating rolls through a shredding device before it can be handled by the extruder.-

The extrudable composition in the. form of small rubbery curds, as obtained by our method, is fed into the hopper of an extrusion machine and extruded at temperatures ranging from about F. to 260 F., depending, for example, on the particularcomposition employed, the wall thickness of the elements, etc. If sealing elements are desired in the form of short tubes or sleeves, the tubing is cut into the desired lengths by a suitable device, such as an automatic cutter as the tubing passes from the extrusion die onto the moving belt. Where sealing elements of the cap'typeare desired, the tubingmay be pinched closed atintervalswhile hot,- asitleaves the extruder. Any suitable arrangement-such as a rotating cam maybe employed to seal the tubing in this manner. It is obvious that various shapes of dies and devicesforpinching and sealingthe extruded shapesmay be employed in forming the sealing elements.

After the sealing elements havebeen-extruded and cut and sealed to theshape anddimensions necessary for sealing the openingior which they are intended, they are placedin a liquid dilater which causes the elements to expand sufficiently to enable themtobe applied readily to the opening. The sealing elements need: not be placed in the dilater immediately after forming and cutting but may be stored andv dilated just previous to using.

Liquids which have been found tobe eifective as dilaters are mixturescontaining a solvent of the polyvinyl chloride plastic and another compound in which the polyvinyl chloride is either insoluble or only slightlysoluble at elevated temperatures. Examples of suitable solvents are ketones, e.,g,, acetone, methyl-ethyl ketone, isophorone, etc. Examples of compounds in which polyvinyl chloride is insoluble or slightly soluble only at elevated temperatures are aromatic hydrocarbons, e. g., benzene, toluene, xylene, ethyl benzene, cumene, and chlorinated derivatives of such aromatic hydrocarbons. Par ticularly good results have been obtained by employing a dilater comprising a mixture of approximately 85 percent xylene and percent methyl ethyl ketone by volume.

The sealing elements may be allowed to remain in the dilater for varying periods of time depending upon the amount of expansion necessary for subsequent application. However, when the above described mixture of xylene and methyl ethyl ketone is employed, nearly maximum swelling is obtained after about two hours immersion. Longer immersion increases the swelling very little, and does not detract from the ultimate properties of the sealing element.

After the sealing element has been applied to the opening to be sealed, the dilater may be allowed to evaporate under ordinary room conditions of temperature and ressure, or the rate of evaporation may be increased by baking at elevated temperatures below the softening point of the resin. As hereinbefore indicated, the sealing elements shrink as the dilater escapes from the plastic composition, producing a tightly fitting seal.

In order that those skilled in the art may better understand how to practice our invention, the following examples are given for purpose of illustration and not by way of limitation:

Example 1 A pigmented plastic composition containing the following ingredients was prepared:

Parts by weight Polyvinyl chloride resin (Geon RF 100) 8000 Zinc oxide 8000 Litharge 160 Monochlorotoluene 5333 Isophorone 2667 The dry ingredients consisting of the polyvinyl chloride resin as the resin component, zinc oxide and litharge were mixed together in a Baker- Perkins mixer and the mixture of monochlorotoluene and isophorone was then added. The

result was a soft wet mix of about the consistency of stiff mortar. This was mixed for approximately ten minutes at room temperature without any visible change. Heat was then applied to the jacket of the mixer, and as the mixture warmed up to approximately 60 0., it became more fluid at first, and then quite rapidly began to gel and stiffen. At this point the heat to the jacket of the mixer was turned off and cold water was admitted to the jacket. The plastic mass advanced rapidly to a stifi rubber consistency, and as it continued to cool, began to break into small rubbery curds. After the mass had been broken up to the desired degree of fineness, the mixer was stopped and the finished compound, in the form of small rubbery curds, ready for extrusion, was removed.

In Example 1, the ratio of temporary plasticizer to resin is 1:1. In the following example this ratio is about 0.75:1.

Example 2 A transparent extrudable composition was prepared as follows:

isophorone 15 Isophorone 30 Monochlorotoluene 90 The slurry of stabilizer was blended with the isophorone and monochlorotoluene and the mixture was then added to the polyvinyl chloride resin in the mixer. The resulting mixture was then mixed for a'short time at a temperature 60 0., and as the mass began to stiifen it was cooled with continued mixing in the same manner as set forth in Example 1. Mixing of the chilled mass was continued until the mass was broken up into fine rubbery curds. The resultin extrudable composition was much lighter in density than the compound resulting in Example 1.

Example The product of Example 1 was extruded in the form of a tube 0.225 inch in diameter. The tube was cut into two-inch segments. These segments, when immersed in a mixture of (by volume) xylene and 15% (by volume) methyl ethyl ketone were swollen to a diameter of approximately 0.3l-inch. This dilated tube was used to join a 0.25-inch copper tube to a concentric 0.375-inch copper tube. The xylene and methyl ethyl ketone evaporated from the sealing tube, causing the sealing tube to grip tightly both of the copper tubes.

What we claim as new and desire to secure by Letters Patent of the United States is:

A method of sealing an opening comprising the steps of providing a sealing element of approximately the dimensions necessary for sealing said opening, said element being composed of a resinous composition comprising, as the resinous component thereof, a mixture of approximately equal parts by weight of a poly- GLENNARD R. LUCAS. RICHARD C. BRYAN.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 1,969,453 Churchill Aug. 7, 1934 1,997,769 Fletcher Apr. 16, 1935 2,027,962 Currie Jan. 14, 1936 2,183,691 Owens Dec. 19, 1939 2,227,682 Wade Jan. 7, 1941 2,236,552 Ushakoif Apr. 1, 1941 2,249,091 Robinson et al. July 15, 1941 2,264,625 Doolittle Dec. 2, 1941 2,316,197 Tucker Apr. 13, 1943 2,338,787

I Ushakoif Jan. 11, 1944 

